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    聚多巴胺包覆磁性纳米粒子的制备及其在测定金银花中绿原酸上的应用

    Preparation of Polydopamine Coated Magnetic Nanoparticles and Its Application of Determination for Chlorogenic Acid in Lonicera Japonica Thunb.

    • 摘要: 以四氧化三铁为磁核,通过原位氧化自聚合技术制备聚多巴胺包覆的磁性纳米粒子(Fe3O4NPs@SiO2@PDA),采用傅里叶变换红外光谱仪、场发射透射电子显微镜、振动样品磁强计进行表征,并采用吸附动力学和吸附等温线考察其对绿原酸的吸附性能。结果显示,Fe3O4NPs@SiO2@PDA对绿原酸的吸附过程符合准二级动力学模型和Langmuir吸附等温模型,最大吸附量为61.1798 mg·g−1,并且可重复使用5次。取0.5 g金银花样品,研磨成粉,用50%(体积分数,下同)甲醇溶液50 mL超声40 min,冷却后过滤,取滤液5 mL,用50%甲醇溶液定容至50 mL。分取3 mL,加入3 mg Fe3O4NPs@SiO2@PDA,用0.5 mol·L−1盐酸溶液调节pH为5,于40 ℃超声振荡20 min,磁铁分离Fe3O4NPs@SiO2@PDA,用水冲洗,再加入2 mL 5%(体积分数)甲酸溶液,超声洗脱10 min,磁铁分离Fe3O4NPs@SiO2@PDA,取上清液过0.22 μm滤膜,采用高效液相色谱法测定滤液中绿原酸的含量。结果显示,绿原酸的质量浓度在20.0~120.0 mg·L−1内与对应的峰面积呈线性关系,测定下限(10S/N)为2.0 mg·L−1。对100.0 mg·L−1绿原酸标准溶液测定6次,测定值的相对标准偏差小于2.0%。按照标准加入法对实际样品进行回收试验,回收率为98.2%~99.1%。方法用于分析实际金银花样品,绿原酸的检出量为13.51~16.45 mg·g−1

       

      Abstract: The polydopamine coated magnetic nanoparticles (Fe3O4NPs@SiO2@PDA) were prepared using ferroferric oxide as the magnetic core through in-situ oxidation self-polymerization technology. The nanoparticles were characterized by Fourier transform infrared spectrometer, field emission transmission electron microscope and vibrating sample magnetometer. The adsorption performance of Fe3O4NPs@SiO2@PDA for chlorogenic acid was investigated by adsorption kinetics and adsorption isotherms. It was showed by the results that the adsorption process of chlorogenic acid by Fe3O4NPs@SiO2@PDA was conformed to the pseudo-second-order kinetic model and Langmuir adsorption isotherm model, with the maximum adsorption capacity of 61.179 8 mg·g−1. The nanoparticles could be reused for 5 times. 0.5 g of Lonicera japonica Thunb. sample was taken and ground into powder, and 50 mL of 50% (volume fraction, the same below) methanol solution was added. The mixture was ultrasonicated for 40 min. After cooling, the solution was filtered. 5 mL of the filtrate was taken and made its volume up to 50 mL with 50% methanol solution. Then 3 mL of the diluted solution was taken, and 3 mg of Fe3O4NPs@SiO2@PDA were added. The pH of the solution was adjusted to 5 with 0.5 mol·L−1 hydrochloric acid solution, and the mixture was ultrasonically oscillated at 40 ℃ for 20 min. The Fe3O4NPs@SiO2@PDA were separated by a magnet and washed with water, and 2 mL of 5% (volume fraction) formic acid solution was added. After ultrasonic elution for 10 min, the Fe3O4NPs@SiO2@PDA were separated by a magnet, and the supernatant was filtered through a 0.22 μm membrane. Chlorogenic acid in the filtrate was determined by high performance liquid chromatography. As shown by the results, linear relationship between values of peak area and mass concentration of chlorogenic acid was found in the range of 20.0−120.0 mg·L−1, with the lower limit of determination (10S/N) of 2.0 mg·L−1. 100.0 mg·L−1 chlorogenic acid standard solution was determined 6 times, and RSDs of the determined values was less than 2.0%. Test for recovery was made by standard addition method on the actual sample, giving results in the range of 98.2%−99.1%. The method was applied to the analysis of actual Lonicera japonica Thunb. samples, and the detection amounts of chlorogenic acid were in the range of 13.51−16.45 mg·g−1.

       

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